Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806043108/ob2088sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806043108/ob2088Isup2.hkl |
CCDC reference: 628039
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.004 Å
- Disorder in main residue
- R factor = 0.023
- wR factor = 0.057
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1 PLAT411_ALERT_2_B Short Inter H...H Contact H9 .. H16B .. 2.08 Ang. PLAT413_ALERT_2_B Short Inter XH3 .. XHn H2 .. H24A .. 1.98 Ang.
Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.61 Ratio PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C25 PLAT301_ALERT_3_C Main Residue Disorder ......................... 12.00 Perc. PLAT411_ALERT_2_C Short Inter H...H Contact H2 .. H23A .. 2.11 Ang. PLAT411_ALERT_2_C Short Inter H...H Contact H11 .. H15B .. 2.13 Ang.
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1996); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN and SHELXL97.
[Rh2(C4H7O2)2cl2(C8H6N2)2]·C2H3N | F(000) = 1504 |
Mr = 752.26 | Dx = 1.813 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 16.561 (2) Å | θ = 12.5–15.0° |
b = 9.301 (3) Å | µ = 1.43 mm−1 |
c = 17.904 (3) Å | T = 193 K |
β = 92.28 (1)° | Prismatic, brown |
V = 2755.6 (11) Å3 | 0.25 × 0.25 × 0.25 mm |
Z = 4 |
Rigaku AFC-7R diffractometer | Rint = 0.024 |
Graphite monochromator | θmax = 27.5°, θmin = 2.3° |
ω/2θ scans | h = −21→21 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→12 |
Tmin = 0.671, Tmax = 0.700 | l = −23→19 |
9725 measured reflections | 3 standard reflections every 150 reflections |
6318 independent reflections | intensity decay: 0.1% |
5471 reflections with I > 2σ(I) |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.023 | H-atom parameters constrained |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0217P)2 + 1.3025P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.002 |
6318 reflections | Δρmax = 0.43 e Å−3 |
385 parameters | Δρmin = −0.54 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00059 (7) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Rh1 | 0.297151 (10) | 0.286791 (18) | 0.512216 (9) | 0.01962 (5) | |
Rh2 | 0.216635 (10) | 0.416186 (17) | 0.600451 (9) | 0.01847 (5) | |
Cl1 | 0.38715 (4) | 0.12991 (7) | 0.43193 (3) | 0.03222 (13) | |
Cl2 | 0.12840 (3) | 0.52447 (7) | 0.70172 (3) | 0.02959 (13) | |
N1 | 0.35761 (11) | 0.4739 (2) | 0.49496 (10) | 0.0246 (4) | |
N2 | 0.29169 (11) | 0.5873 (2) | 0.59267 (11) | 0.0239 (4) | |
C1 | 0.34701 (13) | 0.5944 (3) | 0.53738 (13) | 0.0256 (5) | |
C2 | 0.40966 (14) | 0.4809 (3) | 0.44013 (14) | 0.0338 (6) | |
H1 | 0.4168 | 0.3986 | 0.4097 | 0.041* | |
C3 | 0.45433 (16) | 0.6056 (3) | 0.42575 (16) | 0.0422 (7) | |
H2 | 0.4910 | 0.6055 | 0.3863 | 0.051* | |
C4 | 0.44584 (15) | 0.7256 (3) | 0.46721 (16) | 0.0390 (6) | |
H3 | 0.4763 | 0.8096 | 0.4575 | 0.047* | |
C5 | 0.39050 (14) | 0.7231 (3) | 0.52545 (14) | 0.0309 (5) | |
C6 | 0.37739 (16) | 0.8431 (3) | 0.57103 (16) | 0.0381 (6) | |
H4 | 0.4050 | 0.9309 | 0.5630 | 0.046* | |
C7 | 0.32465 (16) | 0.8315 (3) | 0.62679 (16) | 0.0389 (6) | |
H5 | 0.3159 | 0.9103 | 0.6592 | 0.047* | |
C8 | 0.28315 (15) | 0.7016 (3) | 0.63600 (15) | 0.0320 (5) | |
H6 | 0.2468 | 0.6951 | 0.6756 | 0.038* | |
N3 | 0.21524 (11) | 0.3424 (2) | 0.42928 (10) | 0.0220 (4) | |
N4 | 0.15043 (10) | 0.49610 (19) | 0.51218 (10) | 0.0206 (4) | |
C9 | 0.15594 (12) | 0.4429 (2) | 0.44117 (12) | 0.0207 (4) | |
C10 | 0.21904 (14) | 0.2861 (3) | 0.36130 (13) | 0.0265 (5) | |
H7 | 0.2602 | 0.2177 | 0.3527 | 0.032* | |
C11 | 0.16547 (15) | 0.3222 (3) | 0.30134 (14) | 0.0318 (5) | |
H8 | 0.1694 | 0.2764 | 0.2542 | 0.038* | |
C12 | 0.10820 (15) | 0.4232 (3) | 0.31176 (13) | 0.0314 (5) | |
H9 | 0.0721 | 0.4500 | 0.2716 | 0.038* | |
C13 | 0.10222 (13) | 0.4888 (2) | 0.38273 (13) | 0.0252 (5) | |
C14 | 0.04544 (14) | 0.5963 (3) | 0.39695 (14) | 0.0293 (5) | |
H10 | 0.0088 | 0.6292 | 0.3585 | 0.035* | |
C15 | 0.04406 (14) | 0.6526 (3) | 0.46711 (14) | 0.0305 (5) | |
H11 | 0.0073 | 0.7276 | 0.4777 | 0.037* | |
C16 | 0.09649 (14) | 0.6001 (2) | 0.52325 (14) | 0.0265 (5) | |
H12 | 0.0939 | 0.6401 | 0.5719 | 0.032* | |
O1 | 0.22939 (9) | 0.10743 (17) | 0.53411 (9) | 0.0264 (3) | |
O2 | 0.14437 (9) | 0.23744 (16) | 0.60294 (9) | 0.0240 (3) | |
C17 | 0.16821 (13) | 0.1212 (2) | 0.57396 (13) | 0.0247 (5) | |
C18A | 0.1220 (4) | −0.0147 (5) | 0.5931 (5) | 0.0320 (11) | 0.82 (2) |
H13A | 0.1231 | −0.0815 | 0.5501 | 0.038* | 0.82 (2) |
H14A | 0.1503 | −0.0623 | 0.6362 | 0.038* | 0.82 (2) |
C18B | 0.1126 (17) | −0.005 (3) | 0.5721 (16) | 0.026 (6)* | 0.18 (2) |
H13B | 0.1423 | −0.0880 | 0.5937 | 0.031* | 0.18 (2) |
H14B | 0.0988 | −0.0276 | 0.5191 | 0.031* | 0.18 (2) |
C19 | 0.03525 (15) | 0.0108 (3) | 0.61203 (16) | 0.0359 (6) | |
H16B | 0.0487 | 0.0694 | 0.6570 | 0.043* | 0.18 (2) |
H15B | −0.0004 | 0.0711 | 0.5792 | 0.043* | 0.18 (2) |
H15A | 0.0049 | 0.0463 | 0.5670 | 0.043* | 0.82 (2) |
H16A | 0.0333 | 0.0864 | 0.6508 | 0.043* | 0.82 (2) |
C20A | −0.0052 (5) | −0.1225 (12) | 0.6398 (5) | 0.049 (2) | 0.82 (2) |
H17A | 0.0303 | −0.1696 | 0.6774 | 0.073* | 0.82 (2) |
H18A | −0.0160 | −0.1885 | 0.5979 | 0.073* | 0.82 (2) |
H19A | −0.0562 | −0.0964 | 0.6622 | 0.073* | 0.82 (2) |
C20B | −0.018 (2) | −0.111 (6) | 0.639 (2) | 0.031 (7)* | 0.18 (2) |
H17B | 0.0091 | −0.2035 | 0.6298 | 0.047* | 0.18 (2) |
H18B | −0.0699 | −0.1091 | 0.6108 | 0.047* | 0.18 (2) |
H19B | −0.0263 | −0.1001 | 0.6921 | 0.047* | 0.18 (2) |
O3 | 0.37242 (9) | 0.23225 (18) | 0.60168 (9) | 0.0270 (4) | |
O4 | 0.28844 (9) | 0.32674 (18) | 0.68406 (9) | 0.0261 (3) | |
C21 | 0.35028 (13) | 0.2553 (3) | 0.66724 (13) | 0.0257 (5) | |
C22B | 0.4063 (5) | 0.2096 (11) | 0.7313 (4) | 0.033 (2)* | 0.468 (17) |
H20B | 0.3726 | 0.1812 | 0.7733 | 0.040* | 0.468 (17) |
H21B | 0.4380 | 0.2949 | 0.7478 | 0.040* | 0.468 (17) |
C23B | 0.4661 (7) | 0.0865 (12) | 0.7178 (6) | 0.036 (2) | 0.468 (17) |
H22B | 0.4459 | −0.0046 | 0.7388 | 0.043* | 0.468 (17) |
H23B | 0.4730 | 0.0731 | 0.6636 | 0.043* | 0.468 (17) |
C24B | 0.5455 (6) | 0.1283 (13) | 0.7564 (7) | 0.046 (2) | 0.468 (17) |
H24B | 0.5387 | 0.1336 | 0.8104 | 0.069* | 0.468 (17) |
H25B | 0.5626 | 0.2222 | 0.7379 | 0.069* | 0.468 (17) |
H26B | 0.5866 | 0.0561 | 0.7458 | 0.069* | 0.468 (17) |
C22A | 0.3959 (4) | 0.1786 (9) | 0.7315 (3) | 0.0285 (17)* | 0.532 (17) |
H20A | 0.3666 | 0.0898 | 0.7444 | 0.034* | 0.532 (17) |
H21A | 0.3983 | 0.2417 | 0.7761 | 0.034* | 0.532 (17) |
C23A | 0.4840 (6) | 0.1393 (13) | 0.7093 (5) | 0.044 (2) | 0.532 (17) |
H22A | 0.4811 | 0.0724 | 0.6662 | 0.052* | 0.532 (17) |
H23A | 0.5118 | 0.2277 | 0.6933 | 0.052* | 0.532 (17) |
C24A | 0.5322 (7) | 0.0716 (14) | 0.7716 (6) | 0.054 (3) | 0.532 (17) |
H24A | 0.5055 | −0.0170 | 0.7871 | 0.081* | 0.532 (17) |
H25A | 0.5364 | 0.1383 | 0.8140 | 0.081* | 0.532 (17) |
H26A | 0.5864 | 0.0489 | 0.7550 | 0.081* | 0.532 (17) |
N5 | 0.7197 (2) | 0.3637 (4) | 0.6861 (2) | 0.0752 (9) | |
C25 | 0.7404 (2) | 0.2618 (4) | 0.65753 (19) | 0.0519 (8) | |
C26 | 0.7680 (2) | 0.1345 (4) | 0.6211 (2) | 0.0731 (11) | |
H27 | 0.8090 | 0.0866 | 0.6532 | 0.110* | |
H28 | 0.7914 | 0.1607 | 0.5736 | 0.110* | |
H29 | 0.7223 | 0.0692 | 0.6116 | 0.110* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh1 | 0.01620 (9) | 0.02085 (9) | 0.02194 (9) | −0.00084 (6) | 0.00218 (6) | 0.00294 (7) |
Rh2 | 0.01670 (9) | 0.01828 (9) | 0.02040 (9) | −0.00244 (6) | 0.00047 (6) | 0.00152 (6) |
Cl1 | 0.0282 (3) | 0.0349 (3) | 0.0340 (3) | 0.0053 (2) | 0.0066 (2) | 0.0010 (3) |
Cl2 | 0.0294 (3) | 0.0333 (3) | 0.0263 (3) | −0.0006 (2) | 0.0040 (2) | −0.0027 (2) |
N1 | 0.0189 (9) | 0.0276 (10) | 0.0271 (10) | −0.0046 (8) | −0.0017 (7) | 0.0063 (8) |
N2 | 0.0214 (9) | 0.0231 (10) | 0.0267 (10) | −0.0059 (7) | −0.0040 (8) | 0.0033 (8) |
C1 | 0.0212 (11) | 0.0265 (12) | 0.0285 (12) | −0.0055 (9) | −0.0057 (9) | 0.0085 (9) |
C2 | 0.0259 (12) | 0.0403 (15) | 0.0358 (13) | −0.0050 (11) | 0.0068 (10) | 0.0079 (12) |
C3 | 0.0326 (14) | 0.0507 (17) | 0.0442 (16) | −0.0109 (13) | 0.0121 (12) | 0.0150 (14) |
C4 | 0.0301 (13) | 0.0407 (16) | 0.0460 (16) | −0.0153 (12) | −0.0011 (12) | 0.0182 (13) |
C5 | 0.0266 (12) | 0.0306 (13) | 0.0350 (13) | −0.0080 (10) | −0.0065 (10) | 0.0115 (11) |
C6 | 0.0380 (14) | 0.0275 (13) | 0.0478 (16) | −0.0127 (11) | −0.0103 (12) | 0.0090 (12) |
C7 | 0.0413 (15) | 0.0245 (13) | 0.0503 (16) | −0.0097 (11) | −0.0061 (13) | −0.0038 (12) |
C8 | 0.0302 (13) | 0.0268 (13) | 0.0388 (14) | −0.0060 (10) | −0.0035 (11) | −0.0034 (11) |
N3 | 0.0200 (9) | 0.0225 (9) | 0.0235 (9) | −0.0025 (7) | 0.0018 (7) | 0.0018 (8) |
N4 | 0.0192 (9) | 0.0194 (9) | 0.0232 (9) | −0.0028 (7) | 0.0012 (7) | 0.0022 (7) |
C9 | 0.0193 (10) | 0.0189 (10) | 0.0238 (11) | −0.0027 (8) | 0.0000 (8) | 0.0012 (9) |
C10 | 0.0271 (12) | 0.0286 (12) | 0.0239 (11) | −0.0020 (10) | 0.0034 (9) | −0.0015 (9) |
C11 | 0.0340 (13) | 0.0360 (14) | 0.0253 (12) | −0.0049 (11) | 0.0009 (10) | −0.0031 (10) |
C12 | 0.0325 (13) | 0.0366 (14) | 0.0245 (12) | −0.0043 (11) | −0.0066 (10) | 0.0017 (10) |
C13 | 0.0239 (11) | 0.0243 (12) | 0.0270 (11) | −0.0046 (9) | −0.0017 (9) | 0.0028 (9) |
C14 | 0.0246 (12) | 0.0301 (13) | 0.0325 (13) | 0.0002 (10) | −0.0076 (10) | 0.0050 (10) |
C15 | 0.0286 (12) | 0.0253 (12) | 0.0376 (13) | 0.0061 (10) | −0.0006 (10) | 0.0017 (10) |
C16 | 0.0248 (11) | 0.0239 (12) | 0.0307 (12) | 0.0012 (9) | 0.0010 (9) | −0.0011 (10) |
O1 | 0.0239 (8) | 0.0204 (8) | 0.0355 (9) | −0.0020 (6) | 0.0072 (7) | 0.0009 (7) |
O2 | 0.0200 (7) | 0.0188 (8) | 0.0336 (9) | −0.0043 (6) | 0.0049 (6) | −0.0004 (7) |
C17 | 0.0192 (10) | 0.0223 (11) | 0.0325 (12) | −0.0008 (9) | 0.0011 (9) | 0.0027 (10) |
C18A | 0.031 (2) | 0.0190 (18) | 0.047 (3) | −0.0044 (14) | 0.011 (2) | 0.002 (2) |
C19 | 0.0355 (14) | 0.0318 (14) | 0.0409 (14) | −0.0078 (11) | 0.0072 (11) | −0.0005 (12) |
C20A | 0.040 (4) | 0.031 (3) | 0.078 (4) | −0.008 (3) | 0.034 (3) | −0.011 (2) |
O3 | 0.0207 (8) | 0.0345 (9) | 0.0259 (8) | 0.0018 (7) | 0.0014 (6) | 0.0064 (7) |
O4 | 0.0238 (8) | 0.0304 (9) | 0.0239 (8) | 0.0007 (7) | −0.0007 (6) | 0.0043 (7) |
C21 | 0.0212 (11) | 0.0282 (12) | 0.0276 (12) | −0.0028 (9) | −0.0017 (9) | 0.0048 (10) |
C23B | 0.040 (5) | 0.038 (5) | 0.028 (4) | 0.001 (4) | −0.008 (3) | 0.003 (4) |
C24B | 0.036 (4) | 0.046 (6) | 0.056 (6) | −0.007 (4) | −0.001 (4) | 0.002 (4) |
C23A | 0.035 (4) | 0.052 (6) | 0.043 (4) | 0.012 (4) | 0.000 (3) | 0.022 (4) |
C24A | 0.050 (6) | 0.062 (7) | 0.049 (5) | 0.019 (5) | −0.010 (4) | 0.014 (4) |
N5 | 0.074 (2) | 0.062 (2) | 0.089 (2) | −0.0059 (18) | 0.0016 (19) | 0.0077 (19) |
C25 | 0.0504 (19) | 0.051 (2) | 0.0535 (19) | −0.0125 (16) | −0.0092 (15) | 0.0125 (16) |
C26 | 0.073 (3) | 0.065 (2) | 0.079 (3) | −0.001 (2) | −0.023 (2) | −0.008 (2) |
Rh1—Rh2 | 2.4269 (4) | C17—C18B | 1.49 (3) |
Rh1—Cl1 | 2.5666 (7) | C17—C18A | 1.524 (5) |
Rh1—O1 | 2.0569 (16) | C18A—C19 | 1.508 (6) |
Rh1—O3 | 2.0537 (16) | C18A—H13A | 0.9900 |
Rh1—N1 | 2.0374 (19) | C18A—H14A | 0.9900 |
Rh1—N3 | 2.0377 (18) | C18B—C19 | 1.50 (3) |
Rh2—Cl2 | 2.5784 (7) | C18B—H13B | 0.9900 |
Rh2—O2 | 2.0500 (15) | C18B—H14B | 0.9900 |
Rh2—O4 | 2.0508 (15) | C19—C20A | 1.503 (11) |
Rh2—N2 | 2.0278 (19) | C19—C20B | 1.52 (5) |
Rh2—N4 | 2.0284 (18) | C19—H16B | 0.9900 |
N1—C2 | 1.334 (3) | C19—H15B | 0.9900 |
N1—C1 | 1.369 (3) | C19—H15A | 0.9900 |
N2—C8 | 1.327 (3) | C19—H16A | 0.9900 |
N2—C1 | 1.377 (3) | C20A—H17A | 0.9800 |
C1—C5 | 1.417 (3) | C20A—H18A | 0.9800 |
C2—C3 | 1.405 (4) | C20A—H19A | 0.9800 |
C2—H1 | 0.9500 | C20B—H17B | 0.9800 |
C3—C4 | 1.351 (4) | C20B—H18B | 0.9800 |
C3—H2 | 0.9500 | C20B—H19B | 0.9800 |
C4—C5 | 1.416 (4) | O3—C21 | 1.262 (3) |
C4—H3 | 0.9500 | O4—C21 | 1.267 (3) |
C5—C6 | 1.405 (4) | C21—C22B | 1.507 (8) |
C6—C7 | 1.357 (4) | C21—C22A | 1.527 (7) |
C6—H4 | 0.9500 | C22B—C23B | 1.539 (13) |
C7—C8 | 1.403 (3) | C22B—H20B | 0.9900 |
C7—H5 | 0.9500 | C22B—H21B | 0.9900 |
C8—H6 | 0.9500 | C23B—C24B | 1.511 (15) |
N3—C10 | 1.329 (3) | C23B—H22B | 0.9900 |
N3—C9 | 1.378 (3) | C23B—H23B | 0.9900 |
N4—C16 | 1.337 (3) | C24B—H24B | 0.9800 |
N4—C9 | 1.371 (3) | C24B—H25B | 0.9800 |
C9—C13 | 1.412 (3) | C24B—H26B | 0.9800 |
C10—C11 | 1.406 (3) | C22A—C23A | 1.571 (12) |
C10—H7 | 0.9500 | C22A—H20A | 0.9900 |
C11—C12 | 1.353 (4) | C22A—H21A | 0.9900 |
C11—H8 | 0.9500 | C23A—C24A | 1.486 (13) |
C12—C13 | 1.416 (3) | C23A—H22A | 0.9900 |
C12—H9 | 0.9500 | C23A—H23A | 0.9900 |
C13—C14 | 1.403 (3) | C24A—H24A | 0.9800 |
C14—C15 | 1.362 (4) | C24A—H25A | 0.9800 |
C14—H10 | 0.9500 | C24A—H26A | 0.9800 |
C15—C16 | 1.391 (3) | N5—C25 | 1.136 (5) |
C15—H11 | 0.9500 | C25—C26 | 1.435 (5) |
C16—H12 | 0.9500 | C26—H27 | 0.9800 |
O1—C17 | 1.269 (3) | C26—H28 | 0.9800 |
O2—C17 | 1.269 (3) | C26—H29 | 0.9800 |
Cl1—Rh1—Rh2 | 173.148 (16) | N4—C16—C15 | 123.3 (2) |
O1—Rh1—Rh2 | 87.71 (5) | N4—C16—H12 | 118.4 |
O3—Rh1—Rh2 | 86.96 (5) | C15—C16—H12 | 118.4 |
N1—Rh1—Rh2 | 87.78 (6) | C17—O1—Rh1 | 118.63 (15) |
N3—Rh1—Rh2 | 88.93 (5) | C17—O2—Rh2 | 119.38 (14) |
O1—Rh1—Cl1 | 88.80 (5) | O2—C17—O1 | 125.8 (2) |
O3—Rh1—Cl1 | 87.04 (5) | O2—C17—C18B | 118.4 (11) |
N1—Rh1—Cl1 | 95.79 (6) | O1—C17—C18B | 114.5 (11) |
N3—Rh1—Cl1 | 96.94 (5) | O2—C17—C18A | 116.6 (3) |
O3—Rh1—O1 | 88.27 (7) | O1—C17—C18A | 117.5 (3) |
N1—Rh1—O1 | 175.39 (7) | C19—C18A—C17 | 114.3 (3) |
N3—Rh1—O1 | 89.57 (7) | C19—C18A—H13A | 108.7 |
N1—Rh1—O3 | 92.43 (7) | C17—C18A—H13A | 108.7 |
N3—Rh1—O3 | 175.43 (7) | C19—C18A—H14A | 108.7 |
N3—Rh1—N1 | 89.40 (7) | C17—C18A—H14A | 108.7 |
Cl2—Rh2—Rh1 | 173.172 (16) | H13A—C18A—H14A | 107.6 |
O2—Rh2—Rh1 | 87.04 (5) | C17—C18B—C19 | 117.0 (19) |
O4—Rh2—Rh1 | 87.50 (5) | C17—C18B—H13B | 108.0 |
N2—Rh2—Rh1 | 89.45 (6) | C19—C18B—H13B | 108.0 |
N4—Rh2—Rh1 | 88.20 (5) | C17—C18B—H14B | 108.0 |
O2—Rh2—Cl2 | 87.35 (5) | C19—C18B—H14B | 108.0 |
O4—Rh2—Cl2 | 88.49 (5) | H13B—C18B—H14B | 107.3 |
N2—Rh2—Cl2 | 96.19 (6) | C18A—C19—C20A | 112.7 (5) |
N4—Rh2—Cl2 | 95.79 (5) | C20B—C19—H16B | 105.7 |
O4—Rh2—O2 | 88.69 (6) | C18B—C19—H16B | 105.7 |
N2—Rh2—O2 | 176.45 (7) | C20B—C19—H15B | 105.7 |
N4—Rh2—O2 | 90.93 (7) | C18B—C19—H15B | 105.7 |
N2—Rh2—O4 | 91.68 (7) | H16B—C19—H15B | 106.2 |
N4—Rh2—O4 | 175.69 (7) | C18A—C19—H15A | 109.1 |
N4—Rh2—N2 | 88.44 (7) | C20A—C19—H15A | 109.1 |
C2—N1—C1 | 118.0 (2) | C18A—C19—H16A | 109.1 |
C2—N1—Rh1 | 119.31 (18) | C20A—C19—H16A | 109.1 |
C1—N1—Rh1 | 122.72 (15) | H15A—C19—H16A | 107.8 |
C8—N2—C1 | 118.1 (2) | C19—C20A—H17A | 109.5 |
C8—N2—Rh2 | 120.58 (17) | C19—C20A—H18A | 109.5 |
C1—N2—Rh2 | 120.95 (15) | C19—C20A—H19A | 109.5 |
N1—C1—N2 | 117.58 (19) | C19—C20B—H17B | 109.5 |
N1—C1—C5 | 122.0 (2) | C19—C20B—H18B | 109.5 |
N2—C1—C5 | 120.4 (2) | H17B—C20B—H18B | 109.5 |
N1—C2—C3 | 122.4 (3) | C19—C20B—H19B | 109.5 |
N1—C2—H1 | 118.8 | H17B—C20B—H19B | 109.5 |
C3—C2—H1 | 118.8 | H18B—C20B—H19B | 109.5 |
C4—C3—C2 | 120.9 (2) | C21—O3—Rh1 | 119.59 (14) |
C4—C3—H2 | 119.5 | C21—O4—Rh2 | 119.33 (14) |
C2—C3—H2 | 119.5 | O3—C21—O4 | 125.3 (2) |
C3—C4—C5 | 118.4 (2) | O3—C21—C22B | 117.9 (3) |
C3—C4—H3 | 120.8 | O4—C21—C22B | 116.5 (3) |
C5—C4—H3 | 120.8 | O3—C21—C22A | 117.9 (3) |
C6—C5—C4 | 122.3 (2) | O4—C21—C22A | 116.5 (3) |
C6—C5—C1 | 119.5 (2) | C21—C22B—C23B | 118.1 (6) |
C4—C5—C1 | 118.2 (2) | C21—C22B—H20B | 107.8 |
C7—C6—C5 | 118.9 (2) | C23B—C22B—H20B | 107.8 |
C7—C6—H4 | 120.6 | C21—C22B—H21B | 107.8 |
C5—C6—H4 | 120.6 | C23B—C22B—H21B | 107.8 |
C6—C7—C8 | 119.2 (3) | H20B—C22B—H21B | 107.1 |
C6—C7—H5 | 120.4 | C24B—C23B—C22B | 106.9 (10) |
C8—C7—H5 | 120.4 | C24B—C23B—H22B | 110.3 |
N2—C8—C7 | 123.8 (3) | C22B—C23B—H22B | 110.3 |
N2—C8—H6 | 118.1 | C24B—C23B—H23B | 110.3 |
C7—C8—H6 | 118.1 | C22B—C23B—H23B | 110.3 |
C10—N3—C9 | 117.95 (19) | H22B—C23B—H23B | 108.6 |
C10—N3—Rh1 | 120.86 (16) | C21—C22A—C23A | 110.8 (6) |
C9—N3—Rh1 | 121.16 (14) | C21—C22A—H20A | 109.5 |
C16—N4—C9 | 117.92 (19) | C23A—C22A—H20A | 109.5 |
C16—N4—Rh2 | 119.56 (15) | C21—C22A—H21A | 109.5 |
C9—N4—Rh2 | 122.46 (14) | C23A—C22A—H21A | 109.5 |
N4—C9—N3 | 117.51 (19) | H20A—C22A—H21A | 108.1 |
N4—C9—C13 | 121.0 (2) | C24A—C23A—C22A | 112.6 (9) |
N3—C9—C13 | 121.5 (2) | C24A—C23A—H22A | 109.1 |
N3—C10—C11 | 123.6 (2) | C22A—C23A—H22A | 109.1 |
N3—C10—H7 | 118.2 | C24A—C23A—H23A | 109.1 |
C11—C10—H7 | 118.2 | C22A—C23A—H23A | 109.1 |
C12—C11—C10 | 119.0 (2) | H22A—C23A—H23A | 107.8 |
C12—C11—H8 | 120.5 | C23A—C24A—H24A | 109.5 |
C10—C11—H8 | 120.5 | C23A—C24A—H25A | 109.5 |
C11—C12—C13 | 119.8 (2) | H24A—C24A—H25A | 109.5 |
C11—C12—H9 | 120.1 | C23A—C24A—H26A | 109.5 |
C13—C12—H9 | 120.1 | H24A—C24A—H26A | 109.5 |
C14—C13—C9 | 119.2 (2) | H25A—C24A—H26A | 109.5 |
C14—C13—C12 | 122.8 (2) | N5—C25—C26 | 178.9 (4) |
C9—C13—C12 | 118.0 (2) | C25—C26—H27 | 109.5 |
C15—C14—C13 | 118.5 (2) | C25—C26—H28 | 109.5 |
C15—C14—H10 | 120.7 | H27—C26—H28 | 109.5 |
C13—C14—H10 | 120.7 | C25—C26—H29 | 109.5 |
C14—C15—C16 | 119.9 (2) | H27—C26—H29 | 109.5 |
C14—C15—H11 | 120.0 | H28—C26—H29 | 109.5 |
C16—C15—H11 | 120.0 | ||
O1—Rh1—Rh2—O2 | −8.33 (6) | Rh1—Rh2—N4—C9 | 12.16 (16) |
O3—Rh1—Rh2—O4 | −7.90 (6) | Cl2—Rh2—N4—C9 | −162.28 (15) |
N1—Rh1—Rh2—N2 | −8.76 (7) | C16—N4—C9—N3 | 175.89 (19) |
N3—Rh1—Rh2—N4 | −9.74 (7) | Rh2—N4—C9—N3 | −7.2 (3) |
N3—Rh1—Rh2—N2 | −98.20 (7) | C16—N4—C9—C13 | −4.7 (3) |
O3—Rh1—Rh2—N2 | 83.80 (7) | Rh2—N4—C9—C13 | 172.23 (15) |
O1—Rh1—Rh2—N2 | 172.19 (7) | C10—N3—C9—N4 | 177.41 (19) |
N1—Rh1—Rh2—N4 | 79.70 (7) | Rh1—N3—C9—N4 | −4.7 (3) |
O3—Rh1—Rh2—N4 | 172.25 (7) | C10—N3—C9—C13 | −2.0 (3) |
O1—Rh1—Rh2—N4 | −99.35 (7) | Rh1—N3—C9—C13 | 175.92 (16) |
N1—Rh1—Rh2—O2 | 170.72 (7) | C9—N3—C10—C11 | −0.7 (3) |
N3—Rh1—Rh2—O2 | 81.28 (7) | Rh1—N3—C10—C11 | −178.63 (18) |
O3—Rh1—Rh2—O2 | −96.73 (7) | N3—C10—C11—C12 | 2.3 (4) |
N1—Rh1—Rh2—O4 | −100.46 (7) | C10—C11—C12—C13 | −1.1 (4) |
N3—Rh1—Rh2—O4 | 170.10 (7) | N4—C9—C13—C14 | 3.7 (3) |
O1—Rh1—Rh2—O4 | 80.49 (7) | N3—C9—C13—C14 | −177.0 (2) |
N3—Rh1—N1—C2 | −82.57 (18) | N4—C9—C13—C12 | −176.3 (2) |
O3—Rh1—N1—C2 | 101.62 (18) | N3—C9—C13—C12 | 3.1 (3) |
Rh2—Rh1—N1—C2 | −171.52 (17) | C11—C12—C13—C14 | 178.6 (2) |
Cl1—Rh1—N1—C2 | 14.35 (18) | C11—C12—C13—C9 | −1.5 (3) |
N3—Rh1—N1—C1 | 97.21 (17) | C9—C13—C14—C15 | −0.2 (3) |
O3—Rh1—N1—C1 | −78.61 (17) | C12—C13—C14—C15 | 179.7 (2) |
Rh2—Rh1—N1—C1 | 8.26 (16) | C13—C14—C15—C16 | −2.0 (4) |
Cl1—Rh1—N1—C1 | −165.88 (16) | C9—N4—C16—C15 | 2.5 (3) |
N4—Rh2—N2—C8 | 97.28 (19) | Rh2—N4—C16—C15 | −174.54 (18) |
O4—Rh2—N2—C8 | −87.03 (19) | C14—C15—C16—N4 | 0.9 (4) |
Rh1—Rh2—N2—C8 | −174.51 (18) | N3—Rh1—O1—C17 | −81.10 (17) |
Cl2—Rh2—N2—C8 | 1.63 (18) | O3—Rh1—O1—C17 | 94.87 (17) |
N4—Rh2—N2—C1 | −75.87 (17) | Rh2—Rh1—O1—C17 | 7.84 (16) |
O4—Rh2—N2—C1 | 99.82 (17) | Cl1—Rh1—O1—C17 | −178.06 (17) |
Rh1—Rh2—N2—C1 | 12.34 (16) | N4—Rh2—O2—C17 | 100.11 (17) |
Cl2—Rh2—N2—C1 | −171.52 (16) | O4—Rh2—O2—C17 | −75.59 (17) |
C2—N1—C1—N2 | 178.4 (2) | Rh1—Rh2—O2—C17 | 11.97 (16) |
Rh1—N1—C1—N2 | −1.3 (3) | Cl2—Rh2—O2—C17 | −164.14 (17) |
C2—N1—C1—C5 | −1.3 (3) | Rh2—O2—C17—O1 | −9.6 (3) |
Rh1—N1—C1—C5 | 178.96 (16) | Rh2—O2—C17—C18B | −176.2 (12) |
C8—N2—C1—N1 | 177.5 (2) | Rh2—O2—C17—C18A | 166.2 (4) |
Rh2—N2—C1—N1 | −9.2 (3) | Rh1—O1—C17—O2 | −0.6 (3) |
C8—N2—C1—C5 | −2.9 (3) | Rh1—O1—C17—C18B | 166.4 (12) |
Rh2—N2—C1—C5 | 170.46 (16) | Rh1—O1—C17—C18A | −176.5 (4) |
C1—N1—C2—C3 | 1.2 (4) | O2—C17—C18A—C19 | 27.2 (8) |
Rh1—N1—C2—C3 | −179.0 (2) | O1—C17—C18A—C19 | −156.5 (4) |
N1—C2—C3—C4 | −0.5 (4) | C18B—C17—C18A—C19 | −74 (4) |
C2—C3—C4—C5 | −0.3 (4) | O2—C17—C18B—C19 | −6 (2) |
C3—C4—C5—C6 | −179.6 (3) | O1—C17—C18B—C19 | −174.2 (13) |
C3—C4—C5—C1 | 0.2 (4) | C17—C18A—C19—C20A | −172.8 (6) |
N1—C1—C5—C6 | −179.6 (2) | C17—C18B—C19—C20B | −160 (2) |
N2—C1—C5—C6 | 0.7 (3) | N1—Rh1—O3—C21 | 99.14 (18) |
N1—C1—C5—C4 | 0.6 (3) | O1—Rh1—O3—C21 | −76.31 (17) |
N2—C1—C5—C4 | −179.1 (2) | Rh2—Rh1—O3—C21 | 11.50 (17) |
C4—C5—C6—C7 | −178.6 (2) | Cl1—Rh1—O3—C21 | −165.19 (17) |
C1—C5—C6—C7 | 1.6 (4) | N2—Rh2—O4—C21 | −81.93 (17) |
C5—C6—C7—C8 | −1.7 (4) | O2—Rh2—O4—C21 | 94.53 (17) |
C1—N2—C8—C7 | 2.8 (4) | Rh1—Rh2—O4—C21 | 7.44 (16) |
Rh2—N2—C8—C7 | −170.50 (19) | Cl2—Rh2—O4—C21 | −178.08 (17) |
C6—C7—C8—N2 | −0.5 (4) | Rh1—O3—C21—O4 | −9.3 (3) |
N1—Rh1—N3—C10 | 100.86 (18) | Rh1—O3—C21—C22B | 178.2 (5) |
O1—Rh1—N3—C10 | −83.63 (18) | Rh1—O3—C21—C22A | 163.9 (4) |
Rh2—Rh1—N3—C10 | −171.35 (17) | Rh2—O4—C21—O3 | −0.5 (3) |
Cl1—Rh1—N3—C10 | 5.11 (17) | Rh2—O4—C21—C22B | 172.0 (5) |
N1—Rh1—N3—C9 | −76.97 (17) | Rh2—O4—C21—C22A | −173.8 (4) |
O1—Rh1—N3—C9 | 98.54 (16) | O3—C21—C22B—C23B | −25.5 (13) |
Rh2—Rh1—N3—C9 | 10.82 (15) | O4—C21—C22B—C23B | 161.4 (9) |
Cl1—Rh1—N3—C9 | −172.72 (15) | C22A—C21—C22B—C23B | 68 (2) |
N2—Rh2—N4—C16 | −81.45 (17) | C21—C22B—C23B—C24B | 138.9 (7) |
O2—Rh2—N4—C16 | 102.05 (17) | O3—C21—C22A—C23A | 25.1 (10) |
Rh1—Rh2—N4—C16 | −170.94 (16) | O4—C21—C22A—C23A | −161.1 (7) |
Cl2—Rh2—N4—C16 | 14.62 (16) | C22B—C21—C22A—C23A | −68 (2) |
N2—Rh2—N4—C9 | 101.65 (17) | C21—C22A—C23A—C24A | 176.8 (9) |
O2—Rh2—N4—C9 | −74.85 (16) |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register